scholarly journals On-Chip Electrochemical Analysis Combined with Liquid-Phase Electron Microscopy of Zinc Deposition/Dissolution

Author(s):  
Yuki Sasaki ◽  
Kaname Yoshida ◽  
Akihide Kuwabara ◽  
Yuichi Ikuhara

Abstract Dendrite growth of Zn on the anode of Zn-based rechargeable batteries can cause short-circuiting. To avoid the formation of dendrites, the Zn deposition/dissolution behaviors and their dependence on the electrochemical conditions should be clarified. In this study, in situ transmission electron microscopy (TEM) observations using an electrochemical chip (e-chip) were conducted to visualize the initial stage of the electrodeposition of Zn on an anode. The electrochemical data corresponding to the in situ TEM observations were precisely and extensively analyzed. The combined optimized use of a potentiostat and transmission electron microscope enabled electrochemical electrodes to be isolated completely from the potential of the TEM column. This environment stabilized the electrodeposition process during the in situ TEM observations. Under constant-current mode, the electric potential was varied, resulting in the deposition of various amounts of Zn onto the Pt working electrode. Controlling the surface materials of the electrodes and the electrochemical conditions was important for in situ TEM observations of electrochemical reactions.

Nanoscale ◽  
2019 ◽  
Vol 11 (21) ◽  
pp. 10486-10492 ◽  
Author(s):  
Fu-Chun Chen ◽  
Jui-Yuan Chen ◽  
Ya-Hsuan Lin ◽  
Ming-Yu Kuo ◽  
Yung-Jung Hsu ◽  
...  

The formation of different shapes Au–Cu2O core–shell nanoparticles was investigated by in situ liquid cell transmission electron microscopy (LCTEM).


CORROSION ◽  
10.5006/3457 ◽  
2020 ◽  
Vol 76 (5) ◽  
pp. 464-475 ◽  
Author(s):  
Shravan K. Kairy ◽  
Nick Birbilis

The role of magnesium silicide (Mg2Si) and silicon (Si) particles in the localized corrosion of aluminum (Al) alloys was investigated herein. Sub-micrometer-sized Mg2Si and Si particles were grown in the Al matrix of Al-Mg-Si and Al-Si alloys, respectively, and characterized by transmission electron microscopy (TEM). A quasi in situ TEM technique was used to study an identical location containing Mg2Si or Si particle in the Al matrix, prior to and following a period of immersion in 0.1 M NaCl at pH 6, 2, and 12. At pH 6 and 2, Mg2Si was initially “anodic,” preferentially dealloying via selective dissolution of Mg, resulting in the development of SiO-rich remnants that are electrochemically inert. The SiO-rich remnants at pH 2 physically detached from the Al matrix. Silicon particles were electrochemically inert at pH 6, while “cathodic” at pH 2, dissolving the Al matrix at their periphery. It was observed that copper (Cu) was redeposited on Si particles at pH 2. At pH 12, Mg2Si and Si were “cathodic” to the Al matrix. This study clarifies, and provides new insights into, the characteristics of Al alloy physical manifestation of corrosion associated with Mg2Si and Si at the nanoscale.


2005 ◽  
Vol 907 ◽  
Author(s):  
Amanda K Petford-Long ◽  
Thomas Bromwich ◽  
Amit Kohn ◽  
Victoria Jackson ◽  
Takeshi Kasama ◽  
...  

AbstractOne of the most widely studied types of magnetic nanostructure is that used in devices based on the giant magnetoresistance (GMR) or tunnel magnetoresistance (TMR) phenomena. In order to understand the behaviour of these materials it is important to be able to follow their magnetisation reversal mechanism, and one of the techniques enabling micromagnetic studies at the sub-micron scale is transmission electron microscopy. Two techniques can be used: Lorentz transmission electron microscopy and off-axis electron holography, both of which allow the magnetic domain structure of a ferromagnetic material to be investigated dynamically in real-time with a resolution of a few nanometres. These techniques have been used in combination with in situ magnetizing experiments, to carry out qualitative and quantitative studies of magnetization reversal in a range of materials including spin-tunnel junctions, patterned thin film elements and magnetic antidot arrays. Quantitative analysis of the Lorentz TEM data has been carried out using the transport of intensity equation (TIE) approach.


2006 ◽  
Vol 05 (06) ◽  
pp. 951-958 ◽  
Author(s):  
XUEDONG BAI ◽  
EN GE WANG ◽  
ZHONG LIN WANG

Zinc oxide nanobelts, grown by a solid–vapor phase thermal sublimation process, are stimulating extensive interest because of their semiconducting and piezoelectric properties, diverse functionalities and chemical stability. For nanomanipulation and nanomeasurement of an individual ZnO nanobelts, in situ transmission electron microscopy (TEM) technique is a unique approach. In this paper, mechanical resonance of a single ZnO nanobelt, induced by an alternative electric field, was studied by in situ TEM. Due to the rectangular cross-section of the nanobelt, two fundamental resonance modes have been observed in corresponding to two orthogonal transverse vibration directions, showing the versatile applications of nanobelts as nanocantilevers and nanoresonators. The bending modulus of the ZnO nanobelts was measured to be ~ 52 GPa and the damping time constant of the resonance in vacuum of 10–8 Torr was ~ 1.2 ms. The ZnO nanobelts are promising in potential applications as nanocantilevers, nanoresonators and nanoactuators.


1997 ◽  
Vol 480 ◽  
Author(s):  
K. B. Belay ◽  
M. C. Ridgway ◽  
D. J. Llewellyn

AbstractIn-situ transmission electron microscopy (TEM) has been used to characterize the solidphase epitaxial growth of amorphized GaAs at a temperature of 260°C. To maximize heat transfer from the heated holder to the sample and minimize electron-irradiation induced artifacts, non-conventional methodologies were utilized for the preparation of cross-sectional samples. GaAs (3xI) mm rectangular slabs were cut then glued face-to-face to a size of (6x3) mm stack by maintaining the TEM region at the center. This stack was subsequently polished to a thickness of ~ 200 ýtm. A 3 mm disc was then cut from it using a Gatan ultrasonic cutter. The disc was polished and dimpled on both sides to a thickness of ~15 mimT.h is was ion-beam milled at liquid nitrogen temperature to an electron-transparent layer. From a comparison of in-situ and ex-situ measurements of the recrystallization rate, the actual sample temperature during in-situ characterization was estimated to deviate by ≤ 20°C from that of the heated holder. The influence of electron-irradiated was found to be negligible by comparing the recrystallization rate and microstructure of irradiated and unirradiated regions of comparable thickness. Similarly, the influence of “thin-foil effect” was found to be negligible by comparing the recrystallization rate and microstructure of thick and thin regions, the former determined after the removal of the sample from the microscope and further ion-beam milling of tens of microns of material. In conclusion, the potential influence of artifacts during in-situ TEM can be eliminated by the appropriate choice of sample preparation procedures.


1997 ◽  
Vol 504 ◽  
Author(s):  
V. S. Touboltsev ◽  
E. Johnson ◽  
U. Dahmen ◽  
A. Johansen ◽  
L. Sarholt ◽  
...  

AbstracrSi<110> single crystals were implanted at a temperature of 835 K with 150 keV Pb+ ions to a fluence of 1·1020 m−2 corresponding to an average concentration of 2–3 at%. The implanted samples have been studied by Rutherford Backscattering (RBS)/channeling and transmission electron microscopy (TEM) techniques. In as-implanted samples the main fraction of implanted Pb was located on substitutional sites in the Si matrix thus providing a highly supersaturated solution of Pb in Si. Spontaneous precipitation of Pb, giving rise to formation of nanosized Pb inclusions, was found to take place only in the peak region of the implantation. TEM analysis showed that the Pb precipitates had sizes from about 2 to 20 nm and that they grew in parallel cube orientation relationship with the host matrix. The shape of the inclusions was found to be approximately cuboctahedral with poorly developed {111} and {100} facets.In-situ RBS/channeling heating/cooling experiments on both as-implanted samples and samples previously furnace-annealed at 1175 K showed a distinct melting/solidification hysteresis of the Pb inclusions around the bulk melting point for Pb at 600 K. These results were verified by in-situ TEM heating/cooling experiments on as-implanted samples.


2014 ◽  
Vol 905 ◽  
pp. 56-60
Author(s):  
Dan Feng Qiu ◽  
Yong Jun Xia ◽  
He Qing Ma ◽  
Gang Bu

Graphene-NiO nanocomposites were prepared via a solvothermal method. The nanostructure and morphology of the samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). SEM and TEM results indicated that NiO nanoplates distributed homogeneously on graphene sheets. The electrochemical properties of the samples as active anode materials for lithium-ion batteries were examined by constant current charge-discharge cycling. With graphene as conductive matrix, homogeneous distribution of NiO nanoplates can be ensured and volume changes of thenanocomposite during the charge and discharge processes can be accomodated effectively, which results in good electrochemical performance of the composites.


2010 ◽  
Vol 146-147 ◽  
pp. 1365-1368 ◽  
Author(s):  
Li Mei Cha ◽  
Helmut Clemens ◽  
Gerhard Dehm ◽  
Zao Li Zhang

In-situ heating transmission electron microscopy (TEM) was employed to investigate the initial stage of lamellae formation in a high Nb containing γ-TiAl based alloy. A Ti-45Al-7.5Nb alloy (at %), which was heat treated and quenched in a non-equilibrium state such that the matrix consists of ordered a2 grains, was annealed inside a TEM up to 750 °C. The in-situ TEM study reveals that g laths precipitate in the a2 matrix at ~ 750 °C possessing the classical Blackburn orientation relationship, i.e. (0001)a2 // (111)g and [11-20]a2 // <110]g. The microstructure of the in-situ TEM experiment is compared to results from ex-situ heating and subsequent TEM studies.


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